DE944850C - Method for drying phosgene - Google Patents

Method for drying phosgene

Info

Publication number
DE944850C
DE944850C DEF10923A DEF0010923A DE944850C DE 944850 C DE944850 C DE 944850C DE F10923 A DEF10923 A DE F10923A DE F0010923 A DEF0010923 A DE F0010923A DE 944850 C DE944850 C DE 944850C
Authority
DE
Germany
Prior art keywords
phosgene
water vapor
activated carbon
carbon
dried
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
DEF10923A
Other languages
German (de)
Inventor
Dr Georg Brinkmann
Dr Heinz Wollthan
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Bayer AG
Original Assignee
Bayer AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Bayer AG filed Critical Bayer AG
Priority to DEF10923A priority Critical patent/DE944850C/en
Application granted granted Critical
Publication of DE944850C publication Critical patent/DE944850C/en
Expired legal-status Critical Current

Links

Classifications

    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F24HEATING; RANGES; VENTILATING
    • F24FAIR-CONDITIONING; AIR-HUMIDIFICATION; VENTILATION; USE OF AIR CURRENTS FOR SCREENING
    • F24F3/00Air-conditioning systems in which conditioned primary air is supplied from one or more central stations to distributing units in the rooms or spaces where it may receive secondary treatment; Apparatus specially designed for such systems
    • F24F3/12Air-conditioning systems in which conditioned primary air is supplied from one or more central stations to distributing units in the rooms or spaces where it may receive secondary treatment; Apparatus specially designed for such systems characterised by the treatment of the air otherwise than by heating and cooling
    • F24F3/14Air-conditioning systems in which conditioned primary air is supplied from one or more central stations to distributing units in the rooms or spaces where it may receive secondary treatment; Apparatus specially designed for such systems characterised by the treatment of the air otherwise than by heating and cooling by humidification; by dehumidification
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/70Compounds containing carbon and sulfur, e.g. thiophosgene
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/80Phosgene

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Drying Of Gases (AREA)

Description

Bei bestimmten, technischen Prozessen, in denen Phosgen verwendet wird, z. B. bei der Herstellung von Isocyanaten, erweist es sich als notwendig, auch sehr geringe Mengen von Wasserdampf, die in dem Phosgen enthalten sind, zu entfernen, um Korrosionen an den Metallteilen der benutzten Apparatur zu verhüten.In certain technical processes in which phosgene is used, e.g. B. in manufacture of isocyanates, it turns out to be necessary even very small amounts of water vapor that in which phosgene are contained, to remove corrosion on the metal parts of the used To prevent apparatus.

Phosgen kann mit Hilfe der üblichen Trockenmittel nicht getrocknet werden. So scheidet z. B. Calciumchlorid aus, da feuchtes Phosgen stets Chlorwasserstoff enthält, der das Wasser so fest bindet, daß es ihm durch dieses Mittel nicht entzogen werden kann. Andererseits können auch alkalische Trocknungsmittel, wie z. B. Ätznatron oder Natronkalk nicht verwendet werden, da die an der Oberfläche gebildeten Reaktionsprodukte Carbonat und Chlorid den Zutritt des dampfförmigen Phosgens hemmen bzw. verhindern.Phosgene cannot be dried using the usual drying agents. So separates z. B. Calcium chloride, because moist phosgene always contains hydrogen chloride, which makes the water so solid binds so that it cannot be withdrawn from him by this means. On the other hand you can also use alkaline Desiccants, such as. B. Caustic soda or soda lime cannot be used because the The reaction products formed by carbonate and chloride prevent the access of the vaporous surface Inhibit or prevent phosgene.

Eine Entfernung des Wasserdampfes durch Adsorption an einem hydrophilen Adsorbenten, z. B. Kieselgel, ist bei dem ungünstigen Konzentrationsverhältnis von Wasser zu Phosgen nicht genügend wirksam.Removal of the water vapor by adsorption on a hydrophilic adsorbent, e.g. B. Silica gel is not sufficient with the unfavorable concentration ratio of water to phosgene effective.

Es wurde nun gefunden, daß man Phosgen in einfacher und technisch leicht zu verwirklichender Weise trocknen kann, wenn man die bei geringen Gehalten von Wasserdampf sehr langsam verlaufende hydrolytische Umsetzung des Phosgens zu Kohlensäure und Chlorwasserstoff, wobei also Wasser verbraucht wird, durch Berührung mitIt has now been found that phosgene can be realized in a simple and technically easy way It can be dried in a manner that is very slow with low levels of water vapor hydrolytic conversion of phosgene to carbonic acid and hydrogen chloride, so with Water is consumed by contact with

Claims (2)

Aktivkohle, die hierbei die Hydrolysereaktion katalytisch begünstigt, stark beschleunigt. Es wurde experimentell festgestellt, daß hierfür handelsübliche Dämpfadsorptionskohle in gekörnter Form besonders geeignet ist. Es ist zwar in der Literatur bekannt, daß Phosgen an der Oberfläche von feuchter Aktivkohle hydrolytisch zersetzt wird, so daß bei geringen Wassergehalten der Kohle (z. B. in der Anordnung eines Gasmaskenfilters) ίο bei Belastung mit Phosgen dampfförmiger Chlorwasserstoff durchbricht. Es war aber überraschend, daß die katalytische Beeinflussung der Reaktion des in geringer Konzentration vorhandenen Wasserdampfes mit dem im Überschuß vorhandenen Phosgen an getrockneter Aktivkohle so stark ist, daß die zur Vermeidung jeglicher Korrosion erforderliche vollständige Entfernung des Wasserdampfes aus einem Phosgenstrom im- Bereich der technisch in Frage kommenden Strömungsao geschwindigkeiten erfolgt. Es ergab sich, daß man mit Hilfe einer kleinen mit Aktivkohle gefüllten Säule oder einem Aktivkohlefilter sehr große Mengen von Phosgen wirksam trocknen kann. Die Wirksamkeit der Aktivkohle sollte theoretisch zeitlich unbegrenzt sein, praktisch ist die Dauer der Dienstleistung eines entsprechenden Filters tatsächlich sehr groß. Sie wird' dadurch begrenzt, daß durch Adsorption von spurenweise im Phosgendampf vorhandenen höhermolekularen Verbindungen oder durch nicht vollständige Desorption der Reaktionsprodukte eine Blockierung der aktiven Oberfläche stattfindet. Es ist also" erforderlich, einen Indikator zu verwenden, der das Durchtreten von Wasserdampf in geringster Konzentration bzw. 3& in einer Konzentration, bei der Schaden durch Korrosion wahrnehmbar werden, anzeigt. Hierfür erwies sich blankes Metallblech (Folie), besonders solches aus Aluminium, als geeignet. Der Durchbruch zum Wasserdampf in einer Konzentration, die Korrosionserscheinungen auslösen würde, gibt sich durch eine Trübung der blanken Fläche des Metalles zu erkennen, da feuchtes Phosgen im Gegensatz zu trockenem Phosgen verschiedene Metalle stark angreift (vgl. M. Sartori, Chemie der Kampfstoffe, 1935, S. 55, letzter Absatz). Die Aktivkohle muß dann ersetzt werden bzw. in üblicher Weise regeneriert werden. Die technische Durchführung des Verfahrens kann z. B. so getätigt werden, daß das zu trocknende Phosgen, gegebenenfalls in Mischung mit inerten Gasen, durch einen mit Aktivkohle geeigneter Körnung gefüllten Turm oder Filtertopf geleitet wird, wobei in der Ableitung — durch ein Schauglas sichtbar — blanke Aluminiumfolie als Indikator für den Durchtritt von Wasserdampf angebracht wird. •PATENTANSPRÜCHE:Activated carbon, which catalytically promotes the hydrolysis reaction, is greatly accelerated. It has been found experimentally that commercially available steam adsorption carbon in granular form is particularly suitable for this purpose. It is known in the literature that phosgene is hydrolytically decomposed on the surface of moist activated carbon, so that if the water content of the carbon is low (e.g. in the arrangement of a gas mask filter), vaporous hydrogen chloride breaks through when exposed to phosgene. It was surprising, however, that the catalytic influence on the reaction of the water vapor present in low concentration with the phosgene present in excess of dried activated carbon is so strong that the complete removal of the water vapor from a phosgene stream required to avoid any corrosion is in the range of technically in Question coming flowao speeds takes place. It was found that very large amounts of phosgene can be dried effectively with the aid of a small column filled with activated charcoal or an activated charcoal filter. The effectiveness of the activated carbon should theoretically be unlimited in time, in practice the duration of the service of a corresponding filter is actually very long. It is limited by the fact that the active surface is blocked by adsorption of high molecular weight compounds present in traces in the phosgene vapor or by incomplete desorption of the reaction products. It is therefore necessary to use an indicator that shows the passage of water vapor in the lowest concentration or 3% in a concentration at which damage due to corrosion can be perceived. Bare metal sheet (foil), especially aluminum, proved to be the best choice. The breakthrough to water vapor in a concentration that would trigger signs of corrosion is indicated by a clouding of the bare surface of the metal, since moist phosgene, in contrast to dry phosgene, strongly attacks various metals (cf. M. Sartori, Chemie der Kampfstoffe, 1935, p. 55, last paragraph). The activated carbon must then be replaced or regenerated in the usual way inert gases, is passed through a tower or filter pot filled with activated carbon suitable grain size, whereby in the discharge - through a sight glass visible - bare aluminum foil is attached as an indicator for the passage of water vapor. • PATENT CLAIMS: 1. Verfahren zum Trocknen von Phosgen, dadurch gekennzeichnet, daß man das zu trocknende Phosgen über getrocknete Aktivkohle leitet.1. A method for drying phosgene, characterized in that the to be dried Phosgene passes over dried activated charcoal. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß zur Anzeige des Durchbruches von Wasserdampf durch die Kohleschicht in die Ableitung hinter der Kohleschicht eine blanke Metallfolie sichtbar angebracht wird.2. The method according to claim 1, characterized in that that to indicate the breakthrough of water vapor through the carbon layer in the discharge behind the carbon layer a bare metal foil is visibly attached. Angezogene Druckschriften:Referred publications: M. Sartori, »Chemie der Kampfstoffe«, 1935,M. Sartori, "Chemistry of Warfare Agents", 1935, Fries-West, »Chemical Warf are«, 1921,Fries-West, "Chemical Warf are", 1921, S. 131.P. 131. 609 540 6.56609 540 6.56
DEF10923A 1953-01-24 1953-01-25 Method for drying phosgene Expired DE944850C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEF10923A DE944850C (en) 1953-01-24 1953-01-25 Method for drying phosgene

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE747280X 1953-01-24
DEF10923A DE944850C (en) 1953-01-24 1953-01-25 Method for drying phosgene

Publications (1)

Publication Number Publication Date
DE944850C true DE944850C (en) 1956-06-28

Family

ID=25947496

Family Applications (1)

Application Number Title Priority Date Filing Date
DEF10923A Expired DE944850C (en) 1953-01-24 1953-01-25 Method for drying phosgene

Country Status (1)

Country Link
DE (1) DE944850C (en)

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

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